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Palladium catalyst for hydrogenation reaction of 1, 4-butylene glycol and preparation process thereof

A hydrogenation reaction, palladium catalyst technology, applied in catalyst activation/preparation, hydrogenation preparation, catalyst carrier and other directions, can solve the problems of poisoning, inability to adsorb active metals, high cost of precious metals, and achieve strong dissociative hydrogen absorption capacity, excellent The effect of catalytic hydrogenation activity

Active Publication Date: 2022-05-27
LEIYANG JINYUE SCI & TECH DEV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0003] So far, it is recognized that Lindlar catalyst has the best effect and is most widely used. Lindlar catalyst is formed by adsorbing palladium on a carrier (calcium carbonate or barium sulfate) and adding a small amount of inhibitor (lead acetate or quinoline), but the active ingredient of Lindlar catalyst is mainly Palladium, the high cost of precious metals, restricts its widespread use in industrial applications
Secondly, in view of the different chemical reactivity on different carrier materials, and the carrier can regulate the ability of the catalyst to absorb the reaction gas, but it often occurs poisoning and is reduced, causing the active metal to be unable to adsorb hydrogen in the catalytic reaction, so choose a suitable carrier to design and synthesize the price Catalysts with moderate, stable catalytic performance and high efficiency are the key step

Method used

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  • Palladium catalyst for hydrogenation reaction of 1, 4-butylene glycol and preparation process thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0029] To prepare the modified carrier:

[0030] Step S1, respectively weigh 0.012mol magnesium chloride hexahydrate and 0.007mol aluminum chloride hexahydrate, mix and dissolve in 50mL deionized water, denoted as solution a, respectively weigh 0.033mol sodium hydroxide and 0.017mol sodium carbonate, mix and dissolve in 50mL Deionized water, denoted as solution b, slowly add solution b dropwise to solution a under high-speed stirring, complete the dropwise addition after 30 min, react for 2.5 h, control the pH value of the reaction system to 9, and obtain a gel, which is subjected to Centrifugal washing to neutrality, adding distilled water to it, placing it in a hydrothermal crystallization kettle, crystallizing at 102 °C for 16 h, cooling and washing, drying at 80 °C, and pulverizing to obtain Intermediate 1;

[0031] Step S2, add 2.9mmol 2,3-pyridinedicarboxylic acid and 105mL deionized water to the flask, adjust the pH to 8 with sodium hydroxide solution, add 2.9mmol nicke...

Embodiment 2

[0035] To prepare the modified carrier:

[0036]Step S1, respectively weigh 0.013mol magnesium chloride hexahydrate and 0.008mol aluminum chloride hexahydrate, mix and dissolve in 52mL deionized water, denoted as solution a, respectively weigh 0.034mol sodium hydroxide and 0.018mol sodium carbonate, mix and dissolve in 53mL Deionized water, denoted as solution b, slowly add solution b dropwise to solution a under high-speed stirring, complete the dropwise addition after 30 min, react for 2.5 h, control the pH value of the reaction system to 10, and obtain a gel, which is subjected to Centrifugal washing to neutrality, adding distilled water to it, placing it in a hydrothermal crystallization kettle, crystallization at 104°C for 16 hours, cooling and washing, drying at 80°C, and pulverizing to obtain Intermediate 1;

[0037] Step S2, add 3mmol 2,3-pyridinedicarboxylic acid and 107mL deionized water to the flask, adjust pH to 8 with sodium hydroxide solution, add 3mmol nickel ni...

Embodiment 3

[0041] To prepare the modified carrier:

[0042] Step S1, respectively weigh 0.014mol magnesium chloride hexahydrate and 0.009mol aluminum chloride hexahydrate, mix and dissolve in 55mL deionized water, denoted as solution a, respectively weigh 0.035mol sodium hydroxide and 0.019mol sodium carbonate, mix and dissolve in 55mL Deionized water, denoted as solution b, slowly add solution b dropwise to solution a under high-speed stirring, complete the dropwise addition after 30 minutes, react for 3 hours, control the pH value of the reaction system to 11, obtain gel, and centrifuge the gel Washed to neutrality, added distilled water, placed in a hydrothermal crystallization kettle, crystallized at 105°C for 17h, cooled and washed, dried at 80°C, and pulverized to obtain Intermediate 1;

[0043] Step S2, add 3.1mmol 2,3-pyridinedicarboxylic acid and 110mL deionized water to the flask, adjust the pH to 8 with sodium hydroxide solution, add 3.1mmol nickel nitrate hexahydrate, stir ma...

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PUM

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Abstract

The invention discloses a palladium catalyst for hydrogenation reaction of 1, 4-butylene glycol and a preparation process of the palladium catalyst, and belongs to the technical field of catalysts. The designed and synthesized palladium catalyst comprises the following raw materials: a modified carrier and a chloropalladic acid solution, the modified carrier is synthesized into magnesium-aluminum hydrotalcite by a hydrothermal method, the magnesium-aluminum hydrotalcite and a metal ion solution are blended for an ion replacement reaction to generate nickel-based hydrotalcite with an intercalation structure, sodium silicate is added into a dispersion liquid of the nickel-based hydrotalcite with the intercalation structure, and the nickel-based hydrotalcite with the intercalation structure is prepared. And finally, performing low-temperature plasma operation to highly disperse the nano silicon dioxide on the surface of the hydrotalcite so as to obtain the modified carrier. The palladium catalyst also contains nickel element, so that the high efficiency of hydrogenation reaction is ensured, and the cost is reduced; meanwhile, a SiO2 inert substance is introduced into the hydrotalcite carrier, so that the reduction is reduced, and the poisoning effect is prevented. Low-temperature plasma is used for loading to generate an alloy structure, so that active components are effectively prevented from being gathered and inactivated.

Description

technical field [0001] The invention belongs to the technical field of catalysts, and relates to a palladium catalyst for 1,4-butenediol hydrogenation reaction and a preparation process thereof. Background technique [0002] 1,4-Butenediol (BED) is an important chemical raw material, mainly used as a plasticizer for alkyd resins, a cross-linking agent for synthetic resins and a fungicide, etc. Intermediate, can also be used to make nylon and pharmaceutical products. For a long time, there have been many studies and reports on the selective semi-hydrogenation of alkynes and alkyne derivatives (that is, the products are required to selectively stay in the alkene stage). [0003] So far, it is recognized that Lindlar catalyst has the best effect and is the most widely used. Lindlar catalyst is formed by adsorbing palladium on a carrier (calcium carbonate or barium sulfate) and adding a small amount of inhibitor (lead acetate or quinoline), but the main active component of Lind...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): B01J23/89B01J23/755B01J32/00C07C29/17C07C33/035B01J37/34
CPCB01J23/007B01J23/78B01J23/8946C07C29/17B01J37/349C07C33/035Y02P20/584
Inventor 王宝华高宁宁李泽龙王春良何平英李文菊
Owner LEIYANG JINYUE SCI & TECH DEV
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